CN110592568A - Environment-friendly anti-oxidation liquid for negative current collector and preparation and use methods thereof - Google Patents
Environment-friendly anti-oxidation liquid for negative current collector and preparation and use methods thereof Download PDFInfo
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- CN110592568A CN110592568A CN201910871251.XA CN201910871251A CN110592568A CN 110592568 A CN110592568 A CN 110592568A CN 201910871251 A CN201910871251 A CN 201910871251A CN 110592568 A CN110592568 A CN 110592568A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/52—Treatment of copper or alloys based thereon
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Abstract
The invention discloses an environment-friendly anti-oxidation liquid for a negative current collector, which comprises the following components in parts by weight: 3-6 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 2-4 parts of benzo trinitrobenzene file and 1.5-2.5 parts of tannic acid. The invention has the advantages that the method can be directly used in the existing foil-producing integrated machine, and the oxidation resistance of the copper foil produced in a trial mode can meet the requirement that the copper foil is baked for 10-30 min under the existing condition of 150 ℃, and no oxidation discoloration exists. Baking at 160 deg.C for 10-30 min to obtain foil with slight oxidation discoloration or large-area oxidation discoloration. The surface wettability, tensile strength, elongation and the like of the copper foil meet the requirements of the lithium-ion battery copper foil, and have no difference with the chromium liquid passivated copper foil. The compound system is adopted, the existing chromium liquid passivation system can be partially replaced, various indexes of the copper foil meet requirements, the discharge of chromium liquid is reduced, and the environmental protection pressure is reduced.
Description
Technical Field
The invention relates to a surface passivation treatment technology of an ultrathin electrolytic copper foil, in particular to a chromium-free passivation technology of an ultrathin electrolytic copper foil for a lithium ion battery.
Background
In recent years, the country encourages and develops new energy industries to promote the development of lithium ion power battery. The lithium electrolytic copper foil is widely applied as a negative electrode current collector of the lithium ion battery, and the market demand and the capacity of the lithium electrolytic copper foil are synchronously increased. The quality requirement on the lithium-ion battery copper foil is higher and higher, and the foil surface of the lithium-ion battery copper foil cannot be oxidized and discolored under the high-temperature condition. The traditional anti-oxidation process adopts surface treatment comprising coarsening, solidification, acid washing, water washing, zinc nickel plating and the like, the surface treatment process is long, the existing lithium electro-copper foil is mainly 6-8 mu m, the quality problems of folding, concave-convex points, pressing pits and the like are easy to occur in the continuous rolling process of the surface treatment, the cost rate is reduced, and the cost is increased. The existing foil-producing integrated machine is mainly passivated by adopting chromium liquid, wound after being dried and cut into finished products. The chromium anti-oxidation liquid mainly contains hexavalent chromium which is harmful to human bodies and has carcinogenic risk. Due to the prominent environmental protection problem in recent years, the discharge standard of chromium liquid is strict, the chromium-containing anti-oxidation liquid is discharged, the treatment cost is high, serious pollution is easily caused to water and soil, and once the discharge exceeds the standard, the production stopping risk is brought to a company. Lithium electrolytic copper foil use manufacturers require that the surface of the copper foil is low in chromium content and does not contain elements such as nickel, zinc and the like, a chromium plating anti-oxidation process cannot meet the use requirements of related enterprises, the copper foil can be oxidized and discolored to different degrees when being baked at 150 ℃ for more than 10min, and can be oxidized and discolored when being baked at 160 ℃ for more than 10min, so that the high-temperature oxidation resistance is low. Therefore, the oxidation prevention process of the copper foil needs to be developed towards chromium-free and high oxidation resistance.
Chinese patent publication No. CN107151809B discloses an environment-friendly electrolytic copper foil chromium-free passivation treating fluid and a treating method, which comprises the following raw material components: at least 6-8 compounds of phytic acid, sodium silicate, hydrogen peroxide, sulfuric acid, nitric acid, conductive salt, a stabilizer, a complexing agent and a complexing agent; the complexing agent is sodium citrate or sodium tartrate; the complexing agent is hydroxyethylidene diphosphonic acid, monoethanolamine or sodium perfluorooctyl sulfonate. The passivation solution needs to be carried out under the condition of electrification, and the energy consumption is large. For another example, chinese patent publication No. CN107634228A discloses an electrolytic copper foil chromium-free anti-oxidation technology for lithium ion batteries, in which a raw foil of electrolytic copper foil is stripped by a cathode roller, enters a low-temperature anti-oxidation passivation solution through a guide roller, is soaked in the passivation solution, is squeezed by a squeeze roller, is dried by a high-pressure air knife at normal temperature, and is directly wound. The chromium-free anti-oxidation liquid comprises 0.2-2.0g/L of benzotriazole, 0.1-1.2 g/L of benzoic acid, 0.1-1.0 g/L of propyl acetate and the balance of deionized water, but the chromium-free anti-oxidation liquid has poor high-temperature anti-oxidation performance and can be partially or slightly oxidized after being baked at 150 ℃ for 30 min.
Disclosure of Invention
The technical problem to be solved by the invention is that the chromium anti-oxidation liquid adopted by the existing lithium-ion battery copper foil surface anti-oxidation treatment process contains chromium and has low high-temperature oxidation resistance, so that the environment-friendly negative current collector anti-oxidation liquid and the preparation and use methods thereof are provided.
The technical scheme of the invention is as follows: the environment-friendly anti-oxidation liquid for the negative current collector comprises the following components in parts by weight: 3-6 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 2-4 parts of benzo trinitrobenzene file and 1.5-2.5 parts of tannic acid.
The preparation method of the environment-friendly anti-oxidation liquid for the negative current collector comprises the following steps: mixing 3-6 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 2-4 parts of benzo trinitrobenzene file and 1.5-2.5 parts of tannic acid, and uniformly stirring.
The use method of the environment-friendly anti-oxidation liquid for the negative current collector comprises the following steps: (1) cutting the copper foil with the thickness of 8 mu m which is not oxidized into small square blocks with the size of 100 multiplied by 100, soaking the small square blocks in dilute sulfuric acid, washing the small square blocks with water, extruding the solution and drying the small square blocks; (2) soaking the washed copper foil in the environment-friendly negative current collector anti-oxidation liquid for 8-10 s, taking out the copper foil, extruding the surface liquid, and drying the copper foil by using hot air.
The invention has the advantages that the method can be directly used in the existing foil-producing integrated machine, and the oxidation resistance of the copper foil produced in a trial mode can meet the requirement that the copper foil is baked for 10-30 min under the existing condition of 150 ℃, and no oxidation discoloration exists. Baking at 160 deg.C for 10-30 min to obtain foil with slight oxidation discoloration or large-area oxidation discoloration. The surface wettability, tensile strength, elongation and the like of the copper foil meet the requirements of the lithium-ion battery copper foil, and have no difference with the chromium liquid passivated copper foil. Glucose, nonylphenol polyoxyethylene ether, sodium dodecyl benzene sulfonate, benzotriazole, tannic acid and the like adopt a compound system, the existing chromium liquid passivation system can be partially replaced, various indexes of the copper foil meet the requirements, the discharge of chromium liquid is reduced, and the environmental protection pressure is relieved.
Detailed Description
The technical solution of the present invention is clearly and completely described below with reference to the following embodiments. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments based on the embodiments in the present invention, without any inventive work, will be apparent to those skilled in the art from the following description.
Example 1: the environment-friendly anti-oxidation liquid for the negative current collector comprises the following components in parts by weight: 3 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 2 parts of benzotriazole and 1.5 parts of tannic acid, and the components are mixed and stirred uniformly.
Example 2: the environment-friendly anti-oxidation liquid for the negative current collector comprises the following components in parts by weight: 6 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 4 parts of benzotriazole and 1.5 parts of tannic acid, and the components are mixed and stirred uniformly.
Example 3: the environment-friendly anti-oxidation liquid for the negative current collector comprises the following components in parts by weight: 3 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 4 parts of benzotriazole and 2.5 parts of tannic acid, and the components are mixed and stirred uniformly.
Baking chromium-free anti-oxidation liquid raw materials with different proportions at 150 ℃ and 160 ℃ for 10min, 20min and 30min respectively, cutting the unoxidized 8-micron copper foil into small square blocks of 100 multiplied by 100, soaking in dilute sulfuric acid, washing with water, squeezing the liquid and drying; soaking the washed copper foil in an environment-friendly negative current collector anti-oxidation liquid for 8-10 s, taking out the copper foil, extruding surface liquid, drying the extruded surface liquid with hot air, and recording the change conditions of the rough surface and the smooth surface of the copper foil, wherein the data are shown in the following table:
TABLE 1
As can be seen from the above table, the antioxidant solution obtained by compounding glucose, nonylphenol polyoxyethylene ether, sodium dodecylbenzenesulfonate, benzotriazole and tannic acid has good oxidation resistance at 150 ℃ and 160 ℃.
At present, an electrolytic copper foil all-in-one machine is provided with an anti-oxidation system, copper foil is stripped from a cathode roller, is subjected to power-on passivation by chromium liquid, and is wound after being dried. The improved chromium-free anti-oxidation process can be directly used in the existing equipment without electrifying, and the copper foil passes through the chromium-free passivation solution, is squeezed and dried, and then is wound on a winding roller.
The chromium-free passivation solution is prepared according to the mixture ratio of experiments 10, 11 and 12, test production is carried out according to the production process, and the passivated copper foil is baked for 10-30 min at the temperature of 150 ℃ and 160 ℃.
TABLE 2
As can be seen from Table 2, the anti-oxidation liquid for the environment-friendly negative current collector can be directly used in the existing foil-forming all-in-one machine, and the oxidation resistance of the copper foil produced in a trial mode can meet the requirement that the copper foil is baked for 10-30 min at the existing temperature of 150 ℃ without oxidation discoloration. Baking at 160 deg.C for 10-30 min to obtain foil with slight oxidation discoloration or large-area oxidation discoloration. The surface wettability, tensile strength, elongation and the like of the copper foil meet the requirements of the lithium-ion battery copper foil, and have no difference with the chromium liquid passivated copper foil. Glucose, nonylphenol polyoxyethylene ether, sodium dodecyl benzene sulfonate, benzotriazole, tannic acid and the like adopt a compound system, the existing chromium liquid passivation system can be partially replaced, various indexes of the copper foil meet the requirements, the discharge of chromium liquid is reduced, and the environmental protection pressure is relieved.
Claims (3)
1. The environment-friendly anti-oxidation liquid for the negative current collector is characterized by comprising the following components in parts by weight: 3-6 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 2-4 parts of benzo trinitrobenzene file and 1.5-2.5 parts of tannic acid.
2. The method for preparing the environment-friendly anti-oxidation solution for the negative electrode current collector as claimed in claim 1, which is characterized by comprising the following steps of: mixing 3-6 parts of glucose, 5 parts of nonylphenol polyoxyethylene ether, 3 parts of sodium dodecyl benzene sulfonate, 2-4 parts of benzo trinitrobenzene file and 1.5-2.5 parts of tannic acid, and uniformly stirring.
3. The use method of the environment-friendly anti-oxidation liquid for the negative electrode current collector as claimed in claim 1, which is characterized by comprising the following steps: (1) cutting the copper foil with the thickness of 8 mu m which is not oxidized into small square blocks with the size of 100 multiplied by 100, soaking the small square blocks in dilute sulfuric acid, washing the small square blocks with water, extruding the solution and drying the small square blocks; (2) soaking the washed copper foil in the environment-friendly negative current collector anti-oxidation liquid for 8-10 s, taking out the copper foil, extruding the surface liquid, and drying the copper foil by using hot air.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111962081A (en) * | 2020-08-11 | 2020-11-20 | 湖北工程学院 | Organic phosphonic acid and derivative thereof based copper foil anti-oxidation additive and preparation method thereof |
| CN111962082A (en) * | 2020-08-11 | 2020-11-20 | 湖北工程学院 | Green and environment-friendly copper foil antioxidant and anti-oxidation process using same |
| CN112048721A (en) * | 2020-08-11 | 2020-12-08 | 湖北工程学院 | Azole compound-based copper foil anti-oxidation additive and preparation method thereof |
| CN112095109A (en) * | 2020-08-11 | 2020-12-18 | 湖北工程学院 | Electrolytic copper foil antioxidant |
| CN112095108A (en) * | 2020-08-11 | 2020-12-18 | 湖北工程学院 | Electrolytic copper foil antioxidant and anti-oxidation process using same |
| CN114836744A (en) * | 2022-04-28 | 2022-08-02 | 浙江大学 | Chromium-free passivation solution for copper foil and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111962081A (en) * | 2020-08-11 | 2020-11-20 | 湖北工程学院 | Organic phosphonic acid and derivative thereof based copper foil anti-oxidation additive and preparation method thereof |
| CN111962082A (en) * | 2020-08-11 | 2020-11-20 | 湖北工程学院 | Green and environment-friendly copper foil antioxidant and anti-oxidation process using same |
| CN112048721A (en) * | 2020-08-11 | 2020-12-08 | 湖北工程学院 | Azole compound-based copper foil anti-oxidation additive and preparation method thereof |
| CN112095109A (en) * | 2020-08-11 | 2020-12-18 | 湖北工程学院 | Electrolytic copper foil antioxidant |
| CN112095108A (en) * | 2020-08-11 | 2020-12-18 | 湖北工程学院 | Electrolytic copper foil antioxidant and anti-oxidation process using same |
| CN114836744A (en) * | 2022-04-28 | 2022-08-02 | 浙江大学 | Chromium-free passivation solution for copper foil and preparation method thereof |
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